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dmt acetate solution 'gunk' Options
 
Caacia
#1 Posted : 11/19/2013 8:27:14 AM

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Hi there nexians! Smile
SWIM did a large extraction on a suspected Floribunda and all went relatively well (to the naked eye)
Although when SWIM 'salted out' using vinegar from xylene he accidentally took a thin layer of the NP solvent with him.
now SWIMs run into a predicament, there appears to be some kind of residue submerged in the vinegar just below the layer of xylene. SWIM did not defat due to lack of the solvent and that is why he converted to acetate.
So the question remains what is that gunk? How does he remove the xylene layer given its so thin and how does he remove the gunk suspended in the solution assuming it's not wanted... Or is it?
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Well I don't know, I guess I said it to invoke thought.
 

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DreaMTripper
#2 Posted : 11/19/2013 8:48:28 AM

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There have been a few mentions of vinegar creating a weird substance for some it just dispersed and vanished.
Guess is its something from the vinegar, harmless Im sure. Or it could be dmt acetate Ive read it floats..
As to the layer of xylene either evap it off in a water bath in a well ventilated area or pipette it and the vinegar away into a narrow vessel and try to remove it again.
Report back with the result! What area is the floribunda in? Using phyllodes/stems or bark?
 
Caacia
#3 Posted : 11/19/2013 8:55:39 AM

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I definitely will keep you posted it was using bark off a fallen limb
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Well I don't know, I guess I said it to invoke thought.
 
dooby
#4 Posted : 11/19/2013 12:46:53 PM

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[quote=DreaMTripper] Or it could be dmt acetate Ive read it floats..
[quote]

Surely not...(edit: unless not all dmt-acetate is freebased with a slight excess of NaOH) I re-basefied some vinegar and did naphtha pulls... After adding the base and pulling until exhausted (hot naphtha didn't turn cloudy upon cooling or evap)... These things were still in there at that point - I "wasted" a fair amount of time and solvent to discover that it was "un-pullable" and I got rid of it...

Perhaps some "pure" acetic acid mixed with water to replace store-bought vinegar?
It's relatively cheap and can be obtained in pharmaceutical grade (100% anhydrous)...

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Caacia
#5 Posted : 11/19/2013 2:32:15 PM

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So about 90 mg of sodium carbonate was added into the mixture and mixed thoroughly it became difficult to dissolve but was managed.
It was then stored in the fridge for maybe 2 hours and when it was checked on it had developed a thick layer of crystals at the bottom and the gunk seemingly at the top.

Two more things to state/question.
managed to kick the bottle it was previously in, spilling a substantial amount onto the ground, so that sucked.
And lastly what are the chances that the 'crystals' at the bottom are infanct only sodium carbonate?
(The extraction was on a kilogram of bark)
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Well I don't know, I guess I said it to invoke thought.
 
downwardsfromzero
#6 Posted : 11/19/2013 3:33:20 PM

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Caacia wrote:
So about 90 mg of sodium carbonate was added into the mixture and mixed thoroughly it became difficult to dissolve but was managed.
It was then stored in the fridge for maybe 2 hours and when it was checked on it had developed a thick layer of crystals at the bottom and the gunk seemingly at the top.

Two more things to state/question.
managed to kick the bottle it was previously in, spilling a substantial amount onto the ground, so that sucked.
And lastly what are the chances that the 'crystals' at the bottom are infanct only sodium carbonate?
(The extraction was on a kilogram of bark)

That would be an awful lot of crystals of anything if you only added 90 milligrams of sodium carbonate. Perhaps you meant 90 grams? Rather resembles sodium carbonate given the lack of yellow coloration.

By some strange coincidence, I managed to spill a flask of solvent 3 hours ago, but fortunately all the useful stuff remained at the bottom of the flask.Laughing I called myself some very bad names though!




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― Jacques Bergier, quoting Fulcanelli
 
Caacia
#7 Posted : 11/19/2013 4:06:11 PM

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Actually upon review three 30ml plastic shot glasses worth of sodium carbonate is infact 90grams.
I am however not quite disheartened it seems to me to be an awful lot of sodium carbonate to leave the mixture from the temperature change. It shall be reabsorbed in naphtha this time and do one more acetate conversion before turning to freebase one more time for one last naphtha evap.

I have got to say it feels comforting knowing SWIM is not the only one whom has been a bit clumsy tonight(And I shall always blame it on SWIM)
Well I don't know, I guess I said it to invoke thought.
 
Caacia
#8 Posted : 11/21/2013 3:36:08 PM

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Got the end result last night. After doing another acetate pull after the last I used naphtha and let it evap under a fan by a window.
Although the smell indicate I did infact get some dmt. The quantity is.... Well... Abysmal. Confused
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Well I don't know, I guess I said it to invoke thought.
 
DreaMTripper
#9 Posted : 11/22/2013 6:33:00 AM

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Bark needs good preparation so it can be fully lysed.
Did you grind and powder or have a prolonged soak in pH5 solution?
How old was the material? Chances are if it was lying there a while everything couldve decomposed. Or it wasnt an active tree (or a.floribunda) in the first place. Many reasons why the yields abysmal. Is that what you have active?
Most acacias are also a gamble.
 
Caacia
#10 Posted : 11/22/2013 7:36:39 AM

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Did three acid cooks of a kilo bark shredded to absolute particles. 3litres water one litre vinegar. I know . Should have used more water but I was limited with space.
Each cook was for roughly 2 hours.
I didn't get my hopes up for a number of reasons.
The tree resembled a Floribunda. But was not what I would ideally use. Floribunda it's self is so variable as it is.
Also I figured most of the bark would be too old. But all in all made a good research project.
I will soon post picks of tree for details sake.
Not sure if active, not even sure if that amount would even reach threshold?
Well I don't know, I guess I said it to invoke thought.
 
 
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